反相高效液相色谱法测定4,4′-二羧酸-2,2′-联喹啉的含量
RP-HPLC Determination of 4,4′-Dicarboxy-2,2′-biquinoline
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摘要: 应用反相高效液相色谱法测定了4,4′-二羧酸-2,2′-联喹啉(又名2,2′-联喹啉酸,简写作BCA),作为BCA生产过程的质量控制方法.方法中采用Phenomenex-C18柱(4.6 mm×200 mm,5 μm)作为固定相,采用甲醇与0.05 mol·L-1乙酸钠溶液,以3比7的体积比混合配成的溶液作为流动相,其流速为0.5 mL·min-1,柱温为28 ℃,在330 nm波长处作UV-检测,所测得的峰面积值与BCA质量浓度在0.05~10.0 mg·L-1之间呈线性关系.从同一批产品中取7份试样,按所提出的方法测定其BCA的含量,测得BCA量的平均值为98.62%,7次测定的相对标准偏差为1.65%.Abstract: Reverse-phase HPLC was applied to the determination of 4,4′-dicarboxy-2,2′-biquinoline (or named 2,2′-bicinchoninic acid,abbreviate as BCA) as a method of quality control in course of its production.The phenomenex-C18 column (4.6 mm×200 mm,5 μm) was used as the stationary phase and a mixture of methanol and 0.05 mol·L-1 NaOAc solution,mixed in the ratio of 3 to 7 by volume,was used as the mobile phase at a flow-rate of 0.5 mL·min-1,and with column temperature of 28 ℃.UV-detection was made at the wavelength of 330 nm.Linear relationship between values of peak area and concentration of BCA was obtained in the range of 0.05-10.00 mg·L-1.Seven sample of BCA taken from product of same batch,and contents of BCA were determined by the proposed method.The average content of BCA found was 98.62%,with value of RSD (n=7) to be 1.65%.